反应详情

To a solution of 9C (280 mg, 1.63 mmol) in tetrahydrofuran (5 mL), benzylmagnesium chloride (2M in THF) (1.23 mL, 2.46 mmol) was added dropwise. After 3 hours, 3 mL of 2-butanol was added to the reaction and sodium borohydride (0.5 g) was added to the mixture by portion. The reaction was monitored by LC/Mass until it was done. Methanol (5 mL) was added to the mixture. The organic layer was washed with brine and extracted with ethyl acetate (50 mL twice). The organic layer was dried with Na2SO4, filtered and concentrated. The crude product was purified by flash column (Rf: 0.3, 3% MeOH/DCM) to provide the desired product. MS (m/z) 265 [M+H]+.

1. additionwas added to the mixture by portion
2. washThe organic layer was washed with brine
3. extractionextracted with ethyl acetate (50 mL twice)
4. dry with materialThe organic layer was dried with Na2SO4
5. filtrationfiltered
6. concentrationconcentrated
7. customThe crude product was purified by flash column (Rf: 0.3, 3% MeOH/DCM)